CN102876088A - Preparation method of novel organic acryl-chlorinated titanium dioxide nanoparticles - Google Patents
Preparation method of novel organic acryl-chlorinated titanium dioxide nanoparticles Download PDFInfo
- Publication number
- CN102876088A CN102876088A CN2012104088582A CN201210408858A CN102876088A CN 102876088 A CN102876088 A CN 102876088A CN 2012104088582 A CN2012104088582 A CN 2012104088582A CN 201210408858 A CN201210408858 A CN 201210408858A CN 102876088 A CN102876088 A CN 102876088A
- Authority
- CN
- China
- Prior art keywords
- preparation
- nano
- titanium dioxide
- novel organic
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Abstract
The invention discloses a preparation method of organics and particularly relates to a preparation method of novel organic acryl-chlorinated titanium dioxide nanoparticles. The preparation method includes: dissolving trimesoyl chloride in methylene dichloride to obtain homogeneous solution; dispersing hydrophilic titanium dioxide nano particles in the homogeneous solution; adding triethylamine, and mixing for reaction at the constant temperature of 38 DEG C for 4-24 hours, and after reaction, decompressing and leaching to obtain white solid powder; and rinsing with methylene dichloride, placing the rinsed white solid powder in a vacuum drying oven to obtain the novel organic acryl-chlorinated titanium dioxide nanoparticles. The preparation method has the advantages that the presence of acyl chloride groups enhances activity of the nanoparticles, the surface of each particle is provided with a new function layer so that the particles react with polymers with groups such as amino and hydroxyl to enhance the combining effect; the preparation method is novel, simple to operate and safe in process, reaction progress is easy to control, reagents used are easy to purchase, required devices are simple, and the preparation method is easy for industrial production.
Description
Technical field
The present invention relates to a kind of organic preparation method, specifically refer to a kind of preparation method of novel organic chloride nano-titania particle.
Background technology
Nanoparticle is easy to reunite because particle diameter is very little, and surface energy is high, forms offspring, and nano-TiO
2Itself be the material of strong polarity and the particle of miniaturization, the surface hydrophilic oleophobic, in organic polymer, be difficult to Uniform Dispersion, the space can appear on the interface, when entering, airborne moisture will cause at the interface degraded, the embrittlement of superpolymer in the space, cause material property to descend, affect surface-area effects, volume effect and quantum size effect that its nano particle shows.Therefore the reply nano titanium oxide carries out modification, prevents its reunion and caking, improves its dispersiveness, flowability.
Modification (organic agent and TiO to nano titanium oxide
2The connection of particle surface) mainly contains two kinds of forms: physical adsorption and chemisorption
(1) physical adsorption.Because the organic surface active agent molecule generally is comprised of nonpolar group two portions of hydrophilic polar group and oleophylic, as it and the TiO that polarity is arranged
2During the molecule contact, its polar group just is attracted to TiO
2The surface makes the nonpolar group demonstration affine with other organic mediums outside, thereby makes interfacial tension lowering, impels organic medium to infiltrate in the particle that flocks together, and the air in the space is repelled, and makes TiO
2Particle is separated from each other, and reaches the effect of separation.
(2) chemisorption is carried out the part by chemical reaction to particle surface and is coated, and makes particle surface produce new functional layer.Nano-TiO
2Because the Ti-O bond polarity is very big, the water of surface adsorption dissociates because of polarization, easily forms hydroxyl. this surface hydroxyl can improve TiO
2As the performance of sorbent material and various carriers, for surface modification is provided convenience.Be connected introducing lipophilicity group, TiO with hydroxyl reaction by the organic agent with the lipophilicity group
2Become hydrophobic and oleophylic.
Summary of the invention
The present invention adopts the method for chemisorption that hydrophilic nano titanium dioxide is carried out organic modification, has proposed the preparation technology of pyromellitic trimethylsilyl chloride modified hydrophilic type nano-titania particle.Take pyromellitic trimethylsilyl chloride as modifying agent, with the hydroxyl reaction on hydrophilic nano TiO 2 particles surface it is organised, prepare the modified nano-titanium dioxide particle by following approach:
To contain pyromellitic trimethylsilyl chloride (TMC) is dissolved in the methylene dichloride, then the hydrophilic nano TiO 2 particles is dispersed in the solution, heating in water bath, react at a certain temperature 1-2 hour after, add triethylamine, constant temperature stirs, direct decompress filter got solid particulate, simultaneously with this solid of dichloromethane rinse after reaction ended, put into vacuum drying oven dry, put into moisture eliminator after the taking-up sealing and preserve.
The present invention is achieved by following technical proposals:
A kind of preparation method of novel organic chloride nano-titania particle, its feature may further comprise the steps:
Pyromellitic trimethylsilyl chloride is dissolved in the methylene dichloride, form uniform solution, wherein being mixed with mass concentration is 1.6%～13.3%, then the hydrophilic nano TiO 2 particles is dispersed in the mentioned solution, wherein the dense quality degree of nano titanium oxide in solution is 1.6%～13.3%, after reacting 1～2 hour under 38 ℃, add triethylamine, the mass content of above-mentioned triethylamine is 0.01%～0.02% of solution; Stir 4～24h at 38 ℃ of lower reaction constant temperature again, after reaction ends directly decompress filter get the white powder solid, with this solid of dichloromethane rinse 3～5 times, put into 25 ℃ of degree of vacuum drying oven vacuum-drying 2～4 hours simultaneously, get final product to get this product.
As preferably, react preparation with the nano-titania particle of acid chloride groups with pyromellitic trimethylsilyl chloride and hydrophilic nano TiO 2 particles among the above-mentioned preparation method.
Beneficial effect: the present invention is directed to nano-titania particle dispersion effect in organic phase not good, carry out organically-modified and propose present method to the hydrophilic nano TiO 2 particles, thereby the TMC modified hydrophilic type nano-titania particle that makes is simultaneously with phenyl ring and two kinds of groups of acyl chlorides, improved the dispersion effect of nanoparticle in organic phase, simultaneously, the existence of acid chloride groups has strengthened the activity of nanoparticle, can with the polymer reaction with groups such as amido, hydroxyls, strengthen it in conjunction with effect.
Description of drawings
Fig. 1 modified nano-titanium dioxide and the contrast of unmodified nano titanium oxide infrared spectrum
Embodiment
The below specifies enforcement of the present invention, but protection scope of the present invention is not limited to this:
Embodiment 1
To contain pyromellitic trimethylsilyl chloride (TMC) 2g is dissolved in the 50mL methylene dichloride, then hydrophilic nano TiO 2 particles 2g is dispersed in the solution, add triethylamine 1mL, stir 24h at 38 ℃ of lower constant temperature, direct decompress filter got the white powder solid after reaction ended, use simultaneously this solid of 100mL dichloromethane rinse 5 times, put into 25 ℃ of degree of vacuum drying oven vacuum-drying 2 hours, productive rate is 94%, puts into moisture eliminator after the taking-up sealing and preserves.Unmodified nanoparticle and modified Nano particle diffuse reflectance infrared spectroscopy peak have proved that to such as Fig. 1 modified particle has successfully connected acid chloride groups.
Embodiment 2～11
Changing the isothermal reaction time is 4h, 6h, 8h, 10h, 12h, 14h, 16h, 18h, 20h, 22h, and other operational conditions are all identical with embodiment 1, result such as following table:
| Embodiment | Reaction times | The product outward appearance | Productive rate |
| 2 | 4h | White powder | 70% |
| 3 | 6h | White powder | 73% |
| 4 | 8h | White powder | 76% |
| 5 | 10h | White powder | 78% |
| 6 | 12h | White powder | 79% |
| 7 | 14h | White powder | 84% |
| 8 | 16h | White powder | 85% |
| 9 | 18h | White powder | 87% |
| 10 | 20h | White powder | 87% |
| 11 | 22h | White powder | 89% |
Embodiment 12～14
The charging capacity that changes pyromellitic trimethylsilyl chloride is respectively 1g, 3g and 4g, and other operational conditions are all identical with embodiment 1, result such as following table:
| Embodiment | The TMC charging capacity | The product outward appearance | Productive rate |
| 12 | 1g | White powder | 87% |
| 13 | 3g | White powder | 84% |
| 14 | 4g | White powder | 81% |
Embodiment 15～16
The amount that changes nano-titania particle is 1g, 3g, 4g, and other operational conditions are all identical with embodiment 1, result such as following table:
| Embodiment | Nano-TiO 2 | The product outward appearance | Productive rate |
| 15 | 1g | White powder | 88% |
| 16 | 3g | White powder | 89% |
| 17 | 4g | White powder | 86% |
Claims (2)
1. the preparation method of a novel organic chloride nano-titania particle, its feature may further comprise the steps:
Pyromellitic trimethylsilyl chloride is dissolved in the methylene dichloride, form uniform solution, wherein being mixed with mass concentration is 1.6%～13.3%, then the hydrophilic nano TiO 2 particles is dispersed in the mentioned solution, wherein the dense quality degree of nano titanium oxide in solution is 1.6%～13.3%, after reacting 1～2 hour under 38 ℃, add triethylamine, the mass content of above-mentioned triethylamine is 0.01%～0.02% of solution; Stir 4～24h at 38 ℃ of lower reaction constant temperature again, after reaction ends directly decompress filter get the white powder solid, with this solid of dichloromethane rinse 3～5 times, put into 25 ℃ of degree of vacuum drying oven vacuum-drying 2～4 hours simultaneously, get final product to get this product.
2. the preparation method of a kind of novel organic chloride nano-titania particle according to claim 1 is characterized in that reacting preparation with the nano-titania particle of acid chloride groups with pyromellitic trimethylsilyl chloride and hydrophilic nano TiO 2 particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210408858.2A CN102876088B (en) | 2012-10-24 | 2012-10-24 | Preparation method of novel organic acryl-chlorinated titanium dioxide nanoparticles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210408858.2A CN102876088B (en) | 2012-10-24 | 2012-10-24 | Preparation method of novel organic acryl-chlorinated titanium dioxide nanoparticles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102876088A true CN102876088A (en) | 2013-01-16 |
| CN102876088B CN102876088B (en) | 2014-07-09 |
Family
ID=47477624
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210408858.2A Active CN102876088B (en) | 2012-10-24 | 2012-10-24 | Preparation method of novel organic acryl-chlorinated titanium dioxide nanoparticles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102876088B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104449221A (en) * | 2014-11-24 | 2015-03-25 | 天长市开林化工有限公司 | High-adhesion flame-retardant corrosion-resistant paint |
| CN104449222A (en) * | 2014-11-24 | 2015-03-25 | 天长市开林化工有限公司 | High-adhesion corrosion-resistant modified titanium dioxide paint |
| CN104449220A (en) * | 2014-11-24 | 2015-03-25 | 天长市开林化工有限公司 | Epoxy resin modified paint with high solidification speed |
| CN104449217A (en) * | 2014-11-24 | 2015-03-25 | 天长市开林化工有限公司 | High-strength abrasion-resistant impact-resistant flame retardant coating |
| CN110652750A (en) * | 2019-09-30 | 2020-01-07 | 中国科学院过程工程研究所 | Demulsifier, preparation method and application thereof |
| CN111944304A (en) * | 2020-08-18 | 2020-11-17 | 濮阳市恒信橡塑有限公司 | Polyurethane sealing rubber and preparation method thereof |
| CN115260850A (en) * | 2022-06-30 | 2022-11-01 | 湖南景呈包装有限公司 | Wear-resistant anti-slip carton glazing oil and preparation method and application thereof |
| CN116145280A (en) * | 2022-12-31 | 2023-05-23 | 诸暨市锦晨纺织有限公司 | TiO (titanium dioxide) 2 PHMG composite modified PET antibacterial fabric and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009071332A2 (en) * | 2007-12-06 | 2009-06-11 | Süd-Chemie AG | Nanoparticulate composition and method for the production thereof |
| CN101745325A (en) * | 2008-12-10 | 2010-06-23 | 王志梅 | Method for synthesizing polyesteramide reverse osmosis membrane |
| WO2012102678A1 (en) * | 2011-01-24 | 2012-08-02 | Nano-Mem Pte. Ltd. | A forward osmosis membrane |
-
2012
- 2012-10-24 CN CN201210408858.2A patent/CN102876088B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009071332A2 (en) * | 2007-12-06 | 2009-06-11 | Süd-Chemie AG | Nanoparticulate composition and method for the production thereof |
| CN101745325A (en) * | 2008-12-10 | 2010-06-23 | 王志梅 | Method for synthesizing polyesteramide reverse osmosis membrane |
| WO2012102678A1 (en) * | 2011-01-24 | 2012-08-02 | Nano-Mem Pte. Ltd. | A forward osmosis membrane |
Non-Patent Citations (1)
| Title |
|---|
| 樊晋琼等: "二氧化钛／聚酰胺正渗透复合膜的制备与表征", 《水处理技术》, vol. 38, no. 9, 30 September 2012 (2012-09-30), pages 43 - 46 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104449221A (en) * | 2014-11-24 | 2015-03-25 | 天长市开林化工有限公司 | High-adhesion flame-retardant corrosion-resistant paint |
| CN104449222A (en) * | 2014-11-24 | 2015-03-25 | 天长市开林化工有限公司 | High-adhesion corrosion-resistant modified titanium dioxide paint |
| CN104449220A (en) * | 2014-11-24 | 2015-03-25 | 天长市开林化工有限公司 | Epoxy resin modified paint with high solidification speed |
| CN104449217A (en) * | 2014-11-24 | 2015-03-25 | 天长市开林化工有限公司 | High-strength abrasion-resistant impact-resistant flame retardant coating |
| CN110652750A (en) * | 2019-09-30 | 2020-01-07 | 中国科学院过程工程研究所 | Demulsifier, preparation method and application thereof |
| CN111944304A (en) * | 2020-08-18 | 2020-11-17 | 濮阳市恒信橡塑有限公司 | Polyurethane sealing rubber and preparation method thereof |
| CN115260850A (en) * | 2022-06-30 | 2022-11-01 | 湖南景呈包装有限公司 | Wear-resistant anti-slip carton glazing oil and preparation method and application thereof |
| CN116145280A (en) * | 2022-12-31 | 2023-05-23 | 诸暨市锦晨纺织有限公司 | TiO (titanium dioxide) 2 PHMG composite modified PET antibacterial fabric and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102876088B (en) | 2014-07-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102876088B (en) | Preparation method of novel organic acryl-chlorinated titanium dioxide nanoparticles | |
| Shi et al. | Onion-ring-like g-C3N4 modified with Bi3TaO7 quantum dots: A novel 0D/3D S-scheme heterojunction for enhanced photocatalytic hydrogen production under visible light irradiation | |
| Fronczak et al. | Extraordinary adsorption of methyl blue onto sodium-doped graphitic carbon nitride | |
| Wu et al. | Facile synthesis of Bi2WO6/C3N4/Ti3C2 composite as Z-scheme photocatalyst for efficient ciprofloxacin degradation and H2 production | |
| CN107159133B (en) | Magnetic covalent organic framework material and preparation method and application thereof | |
| Ma et al. | Synthesis of yolk-shell structure Fe3O4/P (MAA-MBAA)-PPy/Au/void/TiO2 magnetic microspheres as visible light active photocatalyst for degradation of organic pollutants | |
| CN109569739A (en) | Double layer hollow material based on titanium dioxide and its application in hydrogen sulfide photocatalysis treatment | |
| CN101224434A (en) | Preparing method of nanometer particle carbon nanotube compound catalyst | |
| CN104588677B (en) | Method for synthesizing shewanella halitios into god nanoparticles and application of gold nanoparticles | |
| CN103301860B (en) | Preparation method of multiwalled carbon nanotube supported silver phosphate visible light photocatalyst | |
| CN105688793A (en) | Preparation method of MnO2-based magnetic nano Fe3O4 heavy metal adsorbing material | |
| CN107308956A (en) | A kind of preparation method of the efficient many iron sulfide of out-phase class fenton catalyst | |
| SG186126A1 (en) | Organic templated nanometal oxyhydroxide | |
| CN109569725A (en) | A kind of method of one-step method preparation magnetism Cu (I) microspherical catalyst | |
| CN105237586A (en) | Preparation and application of novel dual-core organic skeleton material MIL-100(Fe-Mn) | |
| CN109603799A (en) | Graphene/titanic oxide material electrostatic self-assembled preparation method and applications | |
| Khasevani et al. | Green synthesis of ternary carbon dots (CDs)/MIL-88B (Fe)/Bi2S3 nanocomposite via MOF templating as a reusable heterogeneous nanocatalyst and nano-photocatalyst | |
| CN103787344A (en) | Water-soluble mesoporous silica nano-particle and preparation method and application thereof | |
| CN109174194A (en) | A kind of preparation method and applications of the magnetic photocatalytic nano-reactor of degradation selectivity tetracycline | |
| Li et al. | Enhanced photo-catalytic efficiency through dual-functional ZIF based materials: Fabrication and application as a degradation of organic dyes | |
| Wang et al. | Preparation of egg white@ zeolitic imidazolate framework-8@ polyacrylic acid aerogel and its adsorption properties for organic dyes | |
| Esania et al. | Characterization and assessment of the photocatalytic activity of ZnO-Fe3O4/TiO2 nanocomposite based on MIL-125 (Ti) synthesized by mixed solvo-hydrothermal and sol-gel methods | |
| CN103482619B (en) | A kind of Graphene-copper oxide three-dimensional foam composite material | |
| Gopika et al. | A review on current progress of graphene-based ternary nanocomposites in the removal of anionic and cationic inorganic pollutants | |
| CN102275966B (en) | Preparation method of calcium carbonate particulates |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |